Method for preparing pyrazole sulfamide type sodium, potassium and calcium metal complex by ultrasonic wave one-pot method and application
A technology of metal complexes and pyrazole sulfonamides, applied in the direction of calcium organic compounds, sodium organic compounds, potassium organic compounds, etc., to achieve high activity, excellent biological activity, great research and development and application value
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Embodiment 1
[0042] Embodiment 1, the synthesis of sodium complex
[0043]
[0044] Add 1mmol 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole to the flask, then add 25mL ethyl acetate, then slowly add 1.5mmol NaH, Continue to stir for 0.5h after the addition, then dropwise add 1mmol p-toluenesulfonyl chloride, put it into an ultrasonic reactor to react, adjust the power of the ultrasonic reactor to 100W, after 1h, extract with water, remove inorganic salts, collect the organic layer, add Magnesium sulfate water was dried overnight, and a white powder product was obtained by column chromatography. Yield: 86.3%. 1 H-NMR (400MHz, DMSO-d 6 )4.01(q,2H),1.97(s,3H),1.16(t,3H),2.66~2.71(q,2H),1.04~1.08(t,3H); IRν(cm -1 ):2252(ν C≡N ), elemental analysis: according to the theoretical structural formula C 23 h 18 Cl 2 f 6 N 4 NaO 5 S 2 , Calculated: C, 39.38; H, 2.44; N, 7.99%, found: C, 39.79; H, 2.66; N, 8.15%.
[0045] Dissolve the white powder product in ethyl ace...
Embodiment 2
[0056] Embodiment 2, the synthesis of potassium complex
[0057]
[0058] Add 1mmol 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole to the flask, then add 25mL ethyl acetate, then slowly add 1.5mmol KOH, Continue to stir for 0.5h after the addition, then dropwise add 1mmol p-toluenesulfonyl chloride, put it into an ultrasonic reactor for reaction, adjust the power of the ultrasonic reactor to 100W, and after reacting for 2h, extract with water to remove inorganic salts, collect the organic layer, add Anhydrous magnesium sulfate was dried overnight, and a white powder product was obtained by column chromatography. Yield: 85.3%. 1 H-NMR (400MHz, DMSO-d 6 )7.90~7.93(m,4H),4.01(q,2H),1.97(s,3H),1.16(t,3H),2.66~2.71(q,2H),1.04~1.08(t,3H); IRν (cm -1 ):2252(ν C≡N ), elemental analysis: according to the theoretical structural formula C 19 h 9 Cl 2 f 6 KN 4 o 3 S 2 , Calculated: C, 37.22; H, 2.03; N, 8.68%, Found: C, 37.59; H, 2.26; N, 8.89%.
[0059] ...
Embodiment 3
[0068] Embodiment 3, the synthesis of calcium complex
[0069]
[0070] Add 1mmol 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole to the flask, then add 20mL ethyl acetate and 5mL water, then slowly add 1.5 mmol Ca(OH) 2 After the addition, continue to stir for 0.5h, then dropwise add 1mmol p-toluenesulfonyl chloride, put it into an ultrasonic reactor for reaction, adjust the power of the ultrasonic reactor to 100W, and after reacting for 2h, extract with water to remove inorganic salts and collect the organic layer. Anhydrous magnesium sulfate was added to dry overnight, and a white powder product was obtained by column chromatography. Yield: 79.6%. 1 H-NMR (400MHz, DMSO-d 6 )4.02(q,2H),1.98(s,3H),1.17(t,3H),2.62~2.75(q,2H),1.06~1.01(t,3H); IRν(cm -1 ):2254(ν C≡N ). Elemental analysis: according to the theoretical structural formula C 46 h 46 CaCl 4 f 12 N 8 o 16 S 4 , Calculated: C, 36.25; H, 3.72; N, 6.26%, found: C, 36.42; H, 3.96; N, 6.42%....
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